CN117535813A - Flame-retardant lyocell fiber and preparation method thereof - Google Patents
Flame-retardant lyocell fiber and preparation method thereof Download PDFInfo
- Publication number
- CN117535813A CN117535813A CN202311556216.1A CN202311556216A CN117535813A CN 117535813 A CN117535813 A CN 117535813A CN 202311556216 A CN202311556216 A CN 202311556216A CN 117535813 A CN117535813 A CN 117535813A
- Authority
- CN
- China
- Prior art keywords
- lyocell fiber
- flame
- methylmorpholine
- spinning
- retardant lyocell
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000003063 flame retardant Substances 0.000 title claims abstract description 65
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 229920000433 Lyocell Polymers 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- LFTLOKWAGJYHHR-UHFFFAOYSA-N N-methylmorpholine N-oxide Chemical compound CN1(=O)CCOCC1 LFTLOKWAGJYHHR-UHFFFAOYSA-N 0.000 claims abstract description 43
- 238000009987 spinning Methods 0.000 claims abstract description 43
- 229920001131 Pulp (paper) Polymers 0.000 claims abstract description 34
- 239000004114 Ammonium polyphosphate Substances 0.000 claims abstract description 33
- 235000019826 ammonium polyphosphate Nutrition 0.000 claims abstract description 33
- 229920001276 ammonium polyphosphate Polymers 0.000 claims abstract description 33
- 239000000843 powder Substances 0.000 claims abstract description 33
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 26
- ZTHYODDOHIVTJV-UHFFFAOYSA-N Propyl gallate Chemical compound CCCOC(=O)C1=CC(O)=C(O)C(O)=C1 ZTHYODDOHIVTJV-UHFFFAOYSA-N 0.000 claims abstract description 26
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000243 solution Substances 0.000 claims abstract description 23
- 238000005406 washing Methods 0.000 claims abstract description 21
- 239000007864 aqueous solution Substances 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 17
- 229940075579 propyl gallate Drugs 0.000 claims abstract description 13
- 235000010388 propyl gallate Nutrition 0.000 claims abstract description 13
- 239000000473 propyl gallate Substances 0.000 claims abstract description 13
- 238000005520 cutting process Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims description 15
- 239000000835 fiber Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 239000003513 alkali Substances 0.000 abstract description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 13
- 229910052760 oxygen Inorganic materials 0.000 description 13
- 239000001301 oxygen Substances 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 239000011550 stock solution Substances 0.000 description 5
- 239000003921 oil Substances 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000002788 crimping Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000004753 textile Substances 0.000 description 3
- 229920003043 Cellulose fiber Polymers 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N Furan Chemical compound C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 230000015271 coagulation Effects 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 230000008961 swelling Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910001413 alkali metal ion Inorganic materials 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001112 coagulating effect Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- XPPKVPWEQAFLFU-UHFFFAOYSA-N diphosphoric acid Chemical compound OP(O)(=O)OP(O)(O)=O XPPKVPWEQAFLFU-UHFFFAOYSA-N 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 1
- 238000001891 gel spinning Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 239000012796 inorganic flame retardant Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000010665 pine oil Substances 0.000 description 1
- 229920001230 polyarylate Polymers 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 229940005657 pyrophosphoric acid Drugs 0.000 description 1
- 239000004627 regenerated cellulose Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
Abstract
The invention relates to a flame-retardant lyocell fiber and a preparation method thereof, comprising the following steps: s1, concentrating an N-methylmorpholine-N-oxide aqueous solution A until the mass fraction of the N-methylmorpholine-N-oxide is 70-75% to obtain an N-methylmorpholine-N-oxide aqueous solution B; s2, adding propyl gallate, melamine coated ammonium polyphosphate and wood pulp powder into the N-methylmorpholine-N-oxide aqueous solution B, concentrating and uniformly stirring to obtain spinning solution; s3, sequentially spinning, washing, oiling, curling, drying and cutting the spinning solution to obtain the flame-retardant lyocell fiber, wherein the initial LOI of the flame-retardant lyocell fiber reaches 23.8-32.2%, and the LOI of the flame-retardant lyocell fiber still reaches 22.6-29.8% after 10 times of alkaline washing. The flame retardant performance of the lyocell fiber is endowed, and the alkali resistance of the lyocell fiber is further improved.
Description
Technical Field
The invention relates to the technical field of fibers, in particular to a flame-retardant lyocell fiber and a preparation method thereof.
Background
The lyocell fiber is a regenerated cellulose fiber, which is prepared by taking natural plant fiber as a raw material, taking N-methylmorpholine-N-oxide (NMMO) as a solvent and spinning by a dry-wet spinning method, wherein 99.5% of NMMO used in the spinning process can be recycled, and the fiber does not pollute the environment and is known as 'green fiber' in the 21 st century. It not only has the comfort of cotton fiber, soft hand feeling of silk and elegant luster of silk, but also has the mechanical property of comparable chemical fiber. Is widely applied in a plurality of textile fields and belongs to high-grade textile fibers.
The lyocell fiber has a limiting oxygen index of only about 17% as other cellulose fibers, belongs to inflammable materials, has flame retardant property, and can effectively reduce potential safety hazards. At present, the blending method is a mainstream research direction of modification of the lyocell fiber, and related technologies adopt inorganic flame retardants such as ammonium polyphosphate and the like to modify the lyocell fiber, so that the prepared flame-retardant fiber can obtain a relatively excellent flame-retardant effect, and when the addition amount of the ammonium polyphosphate is 20%, the Limiting Oxygen Index (LOI) of the ammonium polyphosphate can reach more than 27%. However, during alkali washing, alkali metal ions can improve the water solubility of ammonium polyphosphate and affect the flame retardant performance of the flame retardant lyocell fiber.
Disclosure of Invention
The invention aims to overcome the technical defects, and provides a flame-retardant lyocell fiber and a preparation method thereof, which solve the technical problem that the flame retardance and alkali resistance of the lyocell fiber in the prior art cannot be balanced.
In order to achieve the technical purpose, the technical scheme provided by the invention is as follows:
in a first aspect, the present invention provides a method for preparing flame retardant lyocell fibers, comprising the steps of: s1, concentrating an N-methylmorpholine-N-oxide aqueous solution A until the mass fraction of the N-methylmorpholine-N-oxide is 70-75% to obtain an N-methylmorpholine-N-oxide aqueous solution B; s2, adding propyl gallate, melamine coated ammonium polyphosphate and wood pulp powder into the N-methylmorpholine-N-oxide aqueous solution B, concentrating and uniformly stirring to obtain spinning solution; and S3, spinning, washing, oiling, curling, drying and cutting the spinning solution in sequence to obtain the flame-retardant lyocell fiber.
In a second aspect, the present invention provides a flame retardant lyocell fiber prepared by the above-described preparation method.
Compared with the prior art, the invention has the beneficial effects that:
according to the preparation method of the flame-retardant lyocell fiber, disclosed by the invention, the melamine coated ammonium polyphosphate is added into the lyocell fiber raw material spinning solution in the original production process engineering of the lyocell fiber to prepare the flame-retardant modified lyocell fiber, and compared with the original lyocell fiber, the melamine coated ammonium polyphosphate modified lyocell fiber has better alkali resistance. And the initial LOI of the flame-retardant lyocell fiber reaches 23.8-32.2%, and after 10 times of alkali washing, the LOI of the flame-retardant lyocell fiber still reaches 22.6-29.8%. The flame retardant performance of the lyocell fiber is endowed, and the alkali resistance of the lyocell fiber is further improved.
Drawings
Fig. 1 is a raman image of flame retardant lyocell fiber carbon residue in example 1 of the present invention.
FIG. 2 is an infrared image of flame retardant lyocell carbon residue in example 1 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
In a first aspect, the invention provides a method for preparing flame retardant lyocell fibers, comprising the following steps:
s1, concentrating a raw material N-methylmorpholine-N-oxide aqueous solution A under a first negative pressure until the mass fraction of the N-methylmorpholine-N-oxide is 70-75% to obtain an N-methylmorpholine-N-oxide aqueous solution B; when the concentration of N-methylmorpholine-N-oxide reaches 70% -75% by negative pressure concentration, the swelling performance of the solvent on wood pulp powder is increased, but the swelling performance is slower, so that the solvent is favorable for completely soaking the wood pulp powder. When the mass fraction of the step is too small, the second concentration time can be greatly prolonged and the energy loss is increased because the wood pulp has the water retention function; when the mass fraction is too large, the wood pulp powder is dissolved, so that a 'core-spun' structure is formed, and the wood pulp powder is unevenly dissolved.
S2, sequentially adding propyl gallate, melamine coated ammonium polyphosphate and wood pulp powder into the concentrated N-methylmorpholine-N-oxide aqueous solution B, stirring, concentrating under negative pressure for the second time, and uniformly stirring to obtain spinning stock solution;
s3, spinning, washing, oiling, curling, drying and cutting the spinning solution in sequence to obtain the flame-retardant lyocell fiber.
Preferably, the mass fraction of the N-methylmorpholine-N-oxide aqueous solution A is 45-55%.
Preferably, in step S2, the concentration is carried out until the mass fraction of the N-methylmorpholine-N-oxide is 88-89%.
Preferably, the N-methylmorpholine-N-oxide aqueous solution A is stirred at a temperature of 90-110 ℃ and concentrated under negative pressure. During negative pressure concentration, the electric heating sleeve is used for heating the heat transfer of the reaction kettle to the required temperature through heat transfer oil, and then the vapor generated in the reaction kettle is pumped out through the vacuum pump, so that the concentration of NMMO in the reaction kettle is improved.
The conditions for the second negative pressure concentration are the same as those for the first negative pressure concentration.
Preferably, the addition amount of the propyl gallate is 0.1-1 per mill of the mass of the wood pulp powder.
Preferably, the addition amount of the melamine coated ammonium polyphosphate is 15-25% of the mass of the wood pulp powder. When the addition amount of the melamine coated ammonium polyphosphate is too small, the flame retardant performance cannot meet the requirement, and when the addition amount is too large, the melamine coated ammonium polyphosphate has poor compatibility with the spinning solution, so that more broken filaments occur, and the influence on the spinning process is larger.
Preferably, in the spinning solution, the solid content of the wood pulp powder is 8-12%.
Preferably, the spinning process is as follows: extruding the spinning solution through a screw, filtering and then entering a spinning system, wherein the temperature is 90-110 ℃.
Preferably, the temperature of the water washing is 70-75 ℃, the time is 2-5 min, the temperature of the oiling is 50-55 ℃, and the time is 3-5 s.
In a second aspect, the invention provides a flame retardant lyocell fiber prepared by the preparation method of any one of the above.
The present invention will be described in further detail with reference to specific examples and comparative examples.
Example 1
Embodiment 1 of the present application provides a method for preparing flame retardant lyocell fiber, comprising the following steps:
(1) Stirring 1L of 50% N-methylmorpholine-N-oxide water solution at 100 ℃, and concentrating under negative pressure for the first time until the mass fraction of N-methylmorpholine-N-oxide is 75%;
(2) Adding propyl gallate, melamine coated ammonium polyphosphate and wood pulp powder into the concentrated N-methylmorpholine-N-oxide, stirring, concentrating under negative pressure for the second time until the mass fraction of the N-methylmorpholine-N-oxide is 89%, and uniformly stirring to obtain spinning stock solution; the addition amount of propyl gallate is 1 per mill of the mass of the wood pulp powder, the addition amount of melamine coated ammonium polyphosphate is 20 percent of the mass of the wood pulp powder, and the solid content of the wood pulp powder in the spinning solution is 10 percent.
(3) Extruding the spinning solution through a screw at the temperature of 100 ℃, filtering, and then entering a spinning system. Wherein the length of the air gap is 7cm, the spinning speed is 50m/min, the aperture of the spinneret plate is 0.095mm, and the ejected silk thread is vertically stretched in the air and enters a coagulating bath (28% NMMO aqueous solution) for shaping; then immersing the mixture into hot water at 70 ℃ for water washing for 3min; then the mixture is immersed in an oil bath (pine oil) with the temperature of 55 ℃ for oiling for 3s. Finally, the alkali-resistant flame-retardant lyocell fiber is prepared through crimping, drying and cutting. The resultant flame retardant lyocell fiber was analyzed for carbon residue after combustion, and the results are shown in fig. 1 and 2.
As can be seen from the Raman spectrum of FIG. 1, at 1370cm -1 And 1587cm -1 The D band of amorphous structural carbon and the G band of graphitic structural carbon appear. The calculated peak area ratio of ID/IG is 3.69, which shows that the fiber has better char forming performance; as can be seen from the IR spectrum of FIG. 2, 3433cm in the figure -1 Stretching vibration of-OH at 1547cm -1 The vibration of the aromatic skeleton is caused by the fact that the fiber pyrolysis products mainly comprise anhydrosugar, furan, aldehyde and the like; 1090cm -1 Characteristic peaks for P-O-C bonds, thus indicating that the present inventionThe pyrophosphoric acid generated by pyrolysis of melamine coated ammonium polyphosphate can promote dehydration of fibers to form a compact carbon layer or a cross-linked reticular polyarylate, so as to protect the fibers and prevent combustion.
Example 2
Embodiment 2 of the present application provides a method for preparing flame retardant lyocell fiber, comprising the following steps:
(1) Stirring 1L of N-methylmorpholine-N-oxide water solution with the mass fraction of 45% at 105 ℃, and concentrating under negative pressure for the first time until the mass fraction of N-methylmorpholine-N-oxide is 75%;
(2) Adding propyl gallate, melamine coated ammonium polyphosphate and wood pulp powder into the concentrated N-methylmorpholine-N-oxide, stirring, concentrating under negative pressure for the second time until the mass fraction of the N-methylmorpholine-N-oxide is 89%, and uniformly stirring to obtain spinning stock solution; the addition amount of propyl gallate is 1 per mill of the mass of the wood pulp powder, the addition amount of melamine coated ammonium polyphosphate is 15 percent of the mass of the wood pulp powder, and the solid content of the wood pulp powder in the spinning solution is 12 percent.
(3) Extruding the spinning solution through a screw at 105 ℃, filtering, and entering a spinning system. Wherein the length of the air gap is 7cm, the spinning speed is 50m/min, the aperture of the spinneret plate is 0.095mm, and the ejected silk thread is vertically stretched in the air and enters into a coagulation bath for forming; then immersing the mixture into hot water at 75 ℃ for water washing for 2min; then immersing in an oil bath with the temperature of 55 ℃ for oiling for 3s. Finally, the alkali-resistant flame-retardant lyocell fiber is prepared through crimping, drying and cutting.
Example 3
Embodiment 3 of the present application provides a method for preparing flame retardant lyocell fiber, comprising the following steps:
(1) Stirring 1L of N-methylmorpholine-N-oxide water solution with the mass fraction of 55% at 95 ℃, and concentrating under negative pressure for the first time until the mass fraction of N-methylmorpholine-N-oxide is 75%;
(2) Adding propyl gallate, melamine coated ammonium polyphosphate and wood pulp powder into the concentrated N-methylmorpholine-N-oxide, stirring, concentrating under negative pressure for the second time until the mass fraction of the N-methylmorpholine-N-oxide is 89%, and uniformly stirring to obtain spinning stock solution; the addition amount of propyl gallate is 1 per mill of the mass of the wood pulp powder, the addition amount of melamine coated ammonium polyphosphate is 25 percent of the mass of the wood pulp powder, and the solid content of the wood pulp powder in the spinning solution is 10 percent.
(3) Extruding the spinning solution through a screw at 95 ℃, filtering and then entering a spinning system. Wherein the length of the air gap is 7cm, the spinning speed is 50m/min, the aperture of the spinneret plate is 0.095mm, and the ejected silk thread is vertically stretched in the air and enters into a coagulation bath for forming; then immersing the mixture into hot water at 70 ℃ for water washing for 2min; then the mixture is immersed in an oil bath with the temperature of 50 ℃ for oiling for 5 seconds. Finally, the alkali-resistant flame-retardant lyocell fiber is prepared through crimping, drying and cutting.
Example 4
The other contents are the same as in example 1. The difference is that the addition amount of melamine coated ammonium polyphosphate is 15% of the mass of the wood pulp powder.
Example 5
Otherwise, the same as in example 1 was conducted except that the amount of melamine coated ammonium polyphosphate added was 25% by mass of the wood pulp powder.
Example 6
Otherwise, the same as in example 2 was conducted except that the amount of melamine coated ammonium polyphosphate added was 20% by mass of the wood pulp powder.
Example 7
Otherwise, the same as in example 3 was conducted except that the amount of melamine coated ammonium polyphosphate added was 20% by mass of the wood pulp powder.
Comparative examples 1 to 3
It differs from example 1 only in that the flame retardant used was replaced by 20% ammonium polyphosphate, silane-coated ammonium polyphosphate, titanate-coated ammonium polyphosphate, respectively.
Comparative example 4
This differs from example 1 only in that no flame retardant was added to the spinning dope.
Testing and evaluation
The flame retardant lyocell fibers prepared in examples 1 to 7 and comparative examples 1 to 4 were respectively tested for limiting oxygen index before and after alkali washing with a sodium carbonate solution having a concentration of 2%, and the different fibers were respectively alkali washed 10 times. The fibers before and after alkali washing were tested for limiting oxygen index according to textile industry standard FZ/T50016-2011. The test results are shown in Table 1.
Table 1 limiting oxygen index of flame retardant lyocell fibers of examples 1 to 7 and comparative examples 1 to 4
As can be seen from Table 1, the flame retardant lyocell fibers obtained in examples 1 to 7 of the present invention were subjected to alkali washing 10 times, and the difference between the obtained limiting oxygen index and the initial limiting oxygen index before alkali washing was small, and was in the range of 0.7 to 2.9%; the comparative example 4 was poor in flame retardant effect without adding a flame retardant; however, in comparative examples 1 to 3, although the initial limiting oxygen index was substantially 27% or more (flame retardant material) after the replacement with other types of flame retardants, the limiting oxygen index was significantly decreased by 4.8% or more after alkali washing, indicating that alkali washing was not resistant.
In the invention, the addition amount of melamine coated ammonium polyphosphate is 15-25% of the mass of the wood pulp powder, the initial limiting oxygen index of the obtained flame-retardant lyocell fiber is 23.8-32.2%, and the limiting oxygen index after 10 times of alkaline washing is 22.6-29.8%.
From examples 2 and 4, it is understood that when the amount of the melamine coated ammonium polyphosphate added is reduced, the flame retardant properties of the obtained flame retardant lyocell fiber are lowered; as can be seen from examples 3 and 5, when the amount of the melamine coated ammonium polyphosphate added was increased, the flame retardant performance of the obtained flame retardant lyocell fiber was significantly improved, but the case of yarn breakage occurred more at this time; therefore, the addition amount of the melamine coated ammonium polyphosphate is preferably 20% of the mass of the wood pulp powder, as can be seen from examples 1, 6 and 7, the situation of broken filaments is basically avoided, and the initial limiting oxygen index and the limiting oxygen index of the obtained flame-retardant lyocell fiber after 10 times of alkali washing are both more than 27%, and exceed the standards of flame-retardant materials.
In summary, the invention provides a flame-retardant lyocell fiber and a preparation method thereof, comprising the following steps: stirring the N-methylmorpholine-N-oxide aqueous solution with the mass fraction of 45-55% at 90-110 ℃, concentrating under negative pressure for the first time until the mass fraction of the N-methylmorpholine-N-oxide is 70-75%, adding propyl gallate, melamine coated ammonium polyphosphate and wood pulp powder into the concentrated N-methylmorpholine-N-oxide, stirring, concentrating under negative pressure for the second time until the mass fraction of the N-methylmorpholine-N-oxide is 88-89%, stirring uniformly to obtain spinning stock solution, and sequentially spinning, washing, oiling, curling, drying and cutting to obtain the flame-retardant lyocell fiber. The preparation method of the invention can improve the alkali resistance of the flame-retardant lyocell fiber.
The above-described embodiments of the present invention do not limit the scope of the present invention. Any other corresponding changes and modifications made in accordance with the technical idea of the present invention shall be included in the scope of the claims of the present invention.
Claims (10)
1. The preparation method of the flame-retardant lyocell fiber is characterized by comprising the following steps of:
s1, concentrating an N-methylmorpholine-N-oxide aqueous solution A until the mass fraction of the N-methylmorpholine-N-oxide is 70-75% to obtain an N-methylmorpholine-N-oxide aqueous solution B;
s2, adding propyl gallate, melamine coated ammonium polyphosphate and wood pulp powder into the N-methylmorpholine-N-oxide aqueous solution B, concentrating and uniformly stirring to obtain spinning solution;
and S3, spinning, washing, oiling, curling, drying and cutting the spinning solution in sequence to obtain the flame-retardant lyocell fiber.
2. The preparation method of the flame-retardant lyocell fiber according to claim 1, wherein the mass fraction of the N-methylmorpholine-N-oxide aqueous solution A is 45-55%.
3. The method for preparing flame retardant lyocell fiber according to claim 1, wherein the concentration in step S2 is performed until the mass fraction of N-methylmorpholine-N-oxide is 88 to 89%.
4. A method of preparing flame retardant lyocell fiber according to claim 3, wherein the concentration in step S1 and step S2 is performed by vacuum concentration.
5. The method for preparing flame-retardant lyocell fiber according to claim 1, wherein the addition amount of propyl gallate is 0.1-1 per mill of the mass of wood pulp powder.
6. The method for preparing flame-retardant lyocell fiber according to claim 1, wherein the addition amount of melamine coated ammonium polyphosphate is 15-25% of the mass of the wood pulp powder.
7. The method for preparing flame retardant lyocell fiber according to claim 1, wherein the solid content of said wood pulp powder in said spinning dope is 8 to 12%.
8. The method for preparing flame retardant lyocell fiber according to claim 1, wherein the spinning process is: extruding the spinning solution through a screw, filtering and then entering a spinning system, wherein the temperature is 90-110 ℃.
9. The method for preparing flame retardant lyocell fiber according to claim 1, wherein the water washing temperature is 70-75 ℃ for 2-5 min, the oiling temperature is 50-55 ℃ for 3-5 s.
10. Flame retardant lyocell fibre obtainable by a process according to any one of claims 1 to 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311556216.1A CN117535813A (en) | 2023-11-17 | 2023-11-17 | Flame-retardant lyocell fiber and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311556216.1A CN117535813A (en) | 2023-11-17 | 2023-11-17 | Flame-retardant lyocell fiber and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117535813A true CN117535813A (en) | 2024-02-09 |
Family
ID=89795378
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311556216.1A Pending CN117535813A (en) | 2023-11-17 | 2023-11-17 | Flame-retardant lyocell fiber and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117535813A (en) |
-
2023
- 2023-11-17 CN CN202311556216.1A patent/CN117535813A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Jiang et al. | A review on raw materials, commercial production and properties of lyocell fiber | |
| Zhang et al. | Regenerated cellulose by the lyocell process, a brief review of the process and properties | |
| CN101492837B (en) | Process for producing bacteria cellulose fibre with high degree of polymerization | |
| CN101307502B (en) | Pineapple leaf fiber preparation method | |
| CA2861172C (en) | Method for stabilizing lignin fiber for further conversion to carbon fiber | |
| US11124900B2 (en) | Method for preparing flame-retardant cellulosic fibers | |
| CN109023621B (en) | Flame-retardant antibacterial wool blended yarn | |
| CN109402774B (en) | Anti-fibrillation cellulose fiber and preparation method thereof | |
| CN109267318B (en) | Flame-retardant lyocell fiber and preparation method thereof | |
| CN113957557B (en) | Efficient flame-retardant lyocell fiber and preparation method thereof | |
| US20210277545A1 (en) | Flame retardant yarn | |
| WO2021001780A1 (en) | Process for upcycling textile waste | |
| CN102677504B (en) | Manufacturing process of antibacterial bamboo pulp used for high-wet-modulus fibre | |
| CN117286609B (en) | Bio-based yarn and vortex spinning preparation method thereof | |
| CN1129680C (en) | Process for production of LYOCELL fiber with bamboo material | |
| CN117535813A (en) | Flame-retardant lyocell fiber and preparation method thereof | |
| CN110699769B (en) | Method for preparing lyocell fibers by using ramie fibers as raw materials | |
| CN109537285B (en) | Method for manufacturing flame-retardant viscose fibers | |
| JPH10331027A (en) | Regenerated cellulose fiber and production thereof | |
| CN115537955B (en) | NMMO solvent-method fungus grass regenerated cellulose fiber and preparation method thereof | |
| CN108138380B (en) | Method of making a precursor yarn | |
| CN109162096B (en) | Method for preparing flame-retardant Lyocell cellulose fiber based on post-treatment method | |
| SE2050820A1 (en) | Method of wet spinning precursor fibers comprising lignin and dissolving pulp, and precursor fibers therefrom | |
| SE539261C2 (en) | A process for the manufacture of a lignin shaped body | |
| CA2987025C (en) | A fiber and a process for the manufacture thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |